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3-Bromobenzyl bromide → 1-Bromo-3-[2,2-bis(ethoxycarbonyl)-2-(p-toluoylamino)ethyl]benzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Bromobenzyl bromide | HCID 69979 | — |
| 反応物 | Diethyl p-toluoylaminomalonate | HCID 17447783 | — |
| 反応物 | Ethanol sodium ethoxide | HCID 23706232 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1-Bromo-3-[2,2-bis(ethoxycarbonyl)-2-(p-toluoylamino)ethyl]benzene | HCID 21866798 | 107.5% |
反応手順
To 100 ml of dry ethanol, 21.45 g of 20% sodium ethoxide-ethanol solution and 17.61 g of diethyl p-toluoylaminomalonate were added and stirred for 30 minutes at room temperature under argon atmosphere. After 15.00 g of 3-bromobenzyl bromide was added dropwise, the reaction solution was stirred for 8 hours at 55° C. and then concentrated. To the residue was added water, and extracted with ethyl acetate. The organic layer was washed with brine and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to provide 29.82 g of the objective compound as yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07144906B2 |
| 出典データセット | uspto-grants-2006_12 |
| ORD ID | ord-23ae2b5fcb95489c892ae4900b66172b |
| 出典メモ | uspto-grants-2006_12 |